反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 150 °C
PROCEDURE
实验过程
A mixture of 2-Chloro-4,6-dimethyl-pyrimidine (92 mg, 0.645 mmol, 1 eq.), 3-aminobenzene boronic acid (100 mg, 0.645 mmol, 1 eq.), Na2CO3 (137 mg, 1.29 mmol, 2 eq.), and Pd(PPh3)2Cl2 (23 mg, 0.032 mmol. 5 mol %) in a 1:1 v/v mixture of CH3CN/H2O (2.6 mL) is purged with N2 for 5 minutes and then heated in a microwave at 150° C. for 5 minutes. After cooling to room temperature, the reaction is diluted with EtOAc and sequentially washed with saturated aqueous NaHCO3 and saturated aqueous NaCl. The organic solution is dried over Na2SO4. After concentration, the residue is purified by silica gel chromatography (1:1 hexanes/EtOAc) to give 3-(4,6-Dimethyl-pyrimidin-2-yl)-phenylamine as a yellow semisolid. [MS: (ES+) 200.1 (M+1)+].
WORKUP
后处理
- customis purged with N2 for 5 minutes
- temperatureAfter cooling to room temperature
- additionthe reaction is diluted with EtOAc
- washsequentially washed with saturated aqueous NaHCO3 and saturated aqueous NaCl
- dry with materialThe organic solution is dried over Na2SO4
- concentrationAfter concentration
- customthe residue is purified by silica gel chromatography (1:1 hexanes/EtOAc)